Method of making anhydrous tin chlorid.



G. BAILLIO. METHOD OF MAKING ANHYDROUS TIN GHLORID. APPLIcATIoN nunJAN.15, 1906.

Patented Feb. 27, 1912 2 buses:

0 AMW 344' we 11 lo I of tin to the manufacturer.

citizen of the United States, residing at To all whom it may concern as.PATENT OFFICE.

GERVAIS BA ILCLIO, OF NIAGARA FALLS, NEW YORK, ASSIGNOR TO CASTNERELECTRO- LYTIC .ALKALI COMPANY, A CORPORATION OF VIRGINIA.

Be it known that I, GERVAIS BAILIiIO,2 1.

Niagara Falls,in the county of Niagara and State of New York, haveinvented certain new and useful'Improvement's in Methods of MakingAnhydrous Tin Chlorid, of which, the following is a full, clear, andexact description.

The primary object of my invention is to provide a continuous processfor converting metallic tin intpanhydrous tln b1chlor1d on a commercialscale; I

Inmanufacturing anhydrous tin bichlorid inthe dry way, i. e. by passingdry chlorin gas over metallic tin, suflicient heat is d eveloped to meltthe tin and in this cond tion a certain percentage of tin combines withthe oxygen of the air, mixed with the chlorin g'as,to form stannic oxid,this causing a loss In carrying out my invention, I avoid any oxidationof the metallic tin by submerging the tin in a quantity of anhydrousliquid, so that the tin is completely covered thereby and afterwardapply chlorin. gas thereto. It is essential to carry out this operationin a water-jacketed kettle or other suitable vessel fitted with steamconnections, as it is of primary importance .that the temperature beunder control. While the tin used may be perfectly pure, it is notnecessary that it should be, as very; satisfactory results have beenobtained from a compound containing about 90% tin, the remainingf10%being composed of lead, iron and 0th impurities.

Carbon tetra-chlorid orany suitable an.-

, hydrous liquid may be employed, as the substance in which the tin' issubmerged, but I prefer to use anhydrous. tin bichlorid for thispurpose. hydrous liquid in which the tin is submerged serves as asealto-protectthe tin from being Specification of Letters Patent.Application filed January 15, 1906. Serial No. 296,095.

The tin bichlorid or the an face of the liquid, this is not absolutelyneeessary,'-for the density of the tin bichlorid .is such that whenworking with'finely dis .vided tin which, has been found to be the mostfavorable condition, the tin" can easily be kept suspended in the liquidby the use of agitators and the action will take place at the surface ofthe liquid.

It is necessary to agitate the tin bichlorid to get the process to work.elficiehtly, both in order to control the temperature and on ac countof the fact that the surface of the submerged tin becomes coated withany impurities that may be present in the tin and thus the action of thechlorin on the tin is retarded. By agitating the mass, the metallicsurface is kept clean and the action proceeds Patented Feb. 27, 191 2-chlorid, or other anhydrous liquid, it attacks the tin contained thereinand sealed thereby and forms additional tin'bichlorid. The latter isperfectly free from moisture, notwithstanding the fact that nioistchlorin gas may be used, and may be drawn off from time to time, Withoutinterfering with the continuityof the process.

In operating my process of making anhydrous tin bichlorid, I employ anapparatus shown in the accompanying drawing.

A is the reaction kettle and-is provided with a water jacket controllingthe temperature of its contents. A v i a a are paddles for agitating thecon' tents of the kettle, fc the chlorininlet, 7) the automatic feed forintroducing the tin, D a settling tank, C a Wash-tower for escapinggases, Gr E and E are stills, provided with condenser H; I is thereceiving tank for the anhydrous tin bichlorid.

In operation, the reaction kettle A is filled to the level of the outlet6 with anhydrous tin bichlorid and a quantity of gen, oxygen and tracesof chlorin. pass out at (2 through the return condenser B and thenthrough the Wash-tower C The volume of anhydrous tin bichlorid in Abeing continually increased by the combination of the chlorin gas andthe metallic tin over-flows through-the outlet 6 into the settling tankD from which it flows When sufiicient impurities have accumulatedimpurities are removed. Ihe pipe purities by distilling it from H intoI. The still G? is provided With an agitator kept in motion duringdistillation and a cock 'through Which the 7 cc :K 7 leading from stillsE, "F and G' to the Wash-tower, is.suppl ie d with ,cocks so that whenthese kettles are being filled with tin bichlorid, the escaping gasespass through the wash-twer. L serves a similar purpose for I.

What I claim is I 1. The continuous process of making anhydrous tinbichlorid, Which,consists in sub merging metallic tin beneath thesurface-of liquid anhydrous stannic chlorid, and a fterward applyingmoist chlorin gas thereto.

2. The continuous process of making anhydrous tin bichlorid, whichconsists in submerging metallic tin beneath the surface of liquidanhydrous stannic chlorid, and afterward continuously introducing moistchlorin gas beneath the surface of the liquid and simultaneouslyagitating the substances under treatment.

In witness whereof, I subscribe my signature, in the presence of twowitnesses.

GERVAIS BAILLIO.

Witnesses:

H. H. HACKENHEIMER,

S. N. LEE.

